CN104054156A - Differential ion mobility spectrometer - Google Patents
Differential ion mobility spectrometer Download PDFInfo
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- CN104054156A CN104054156A CN201380004790.4A CN201380004790A CN104054156A CN 104054156 A CN104054156 A CN 104054156A CN 201380004790 A CN201380004790 A CN 201380004790A CN 104054156 A CN104054156 A CN 104054156A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/622—Ion mobility spectrometry
- G01N27/624—Differential mobility spectrometry [DMS]; Field asymmetric-waveform ion mobility spectrometry [FAIMS]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7206—Mass spectrometers interfaced to gas chromatograph
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
The invention relates to the field of gas analysis and is intended to detect trace impurities in gaseous media, specifically in atmospheric air, and can be used in gas chromatography as a sensitive detector. The technical result consists in improving the consistency and repeatability of the results of analyses of gaseous media and extending the service life of an ionizer. The differential ion mobility spectrometer comprises a cylindrical chamber for the formation of analyte ions, an ionization source around which reactant ions are formed, a system of electrodes, an ion aperture, an analytical gap formed between two concentric cylindrical electrodes, an ion registration unit, a generator of periodic voltage with asymmetric polarity which provides an outlet to an area of nonlinear field dependence of ion mobility, a source of compensating voltage, a source of high-frequency voltage which provides for increased resolution of the device, and an additional (third) chamber positioned concentrically in relation to an inner cylindrical electrode, said chamber having an inlet and an outlet for ionizing gas and containing an ionization source and an expulsion force generator; the generator of periodic voltage with asymmetric polarity which provides an outlet to an area of nonlinear field dependence of ion mobility, the source of compensating voltage and the high-frequency voltage generator which provides for increased resolution of the device are connected to the inner electrode of the ionization chamber. The source of ionization may be: a radiation source, or an electronic ionizer, or an electrospray device, or any known source of ultraviolet radiation. A gas purification system is also provided.
Description
Technical field
The present invention relates to gas analysis field, and be intended to detect the trace impurity of in gaseous medium (particularly in atmospheric air), and it can be used as sensitive detectors in gas chromatography.
Background technology
In order to monitor the trace impurity of the organic and inorganic pollution in gas, due to high sensitivity, selectivity and the rapidity analyzed, use the instrument operating as basis taking ionic mobility detection technique.
Prior art is known in disclosed U.S. Patent No. 5420424 on May 30 nineteen ninety-five, IPC H01J49/40, this patent discloses a kind of non-linear ion drift frequency spectrograph, this non-linear ion drift frequency spectrograph comprises: ionization chamber, has and receive the import of gas to be analyzed and discharge the outlet of analytical gas; Ionization source; Electrode system; Ion eyelet; Ion isolation chamber (analytical gap), is limited by two relative electrodes, and ion isolation chamber has purge gas inlet, and is communicated with described ionization chamber by ion eyelet in its import department, and is communicated with ion monitoring device in its exit; Asymmetrical pole alternate voltage-changing generator and compensating voltage source, be both connected to split cavity electrode; Voltage source, is connected to ionization chamber electrode.
When ionization when occur under atmospheric pressure, this prior art equipment presents low sensitivity and low interference immunity, and this low sensitivity and low interference immunity generate for the impact of ionization and the validity separating by being present in pollutant in gas to be analyzed.
In order to solve the one in these defects, solve low interference immunity, once proposed to make this frequency spectrograph be supplemented with gas purge system, this gas purge system is communicated with discharge pipe and split cavity outlet in its import department, and is also communicated with the import of ionization chamber in its exit.Such equipment is disclosed in the U.S. Patent No. 5736739 of delivering on April 7th, 1998, in IPC H01J49/40.
But, so supplementary impact of failing the validity of destroy contaminants on ionization, thereby the sensitivity of impact analysis adversely.
In order to improve the sensitivity of analysis, once proposed to make this frequency spectrograph be supplemented with heated chamber and controlled gas exhausting device.Heated chamber is arranged in the import of ionization chamber, thereby be communicated with analyzed gas and gas purge system outlet in its import department, and be also communicated with the import of ionization chamber in its exit, and it comprises thermometer, heat control unit and hygrometer, this hygrometer is connected to controlled gas exhausting device.This frequency spectrograph is disclosed in the disclosed patent No.2178929 of the Russian Federation on January 27th, 2002, in IPC H01J49/40.
Defect by the known this equipment of prior art is that it can not solve the problem that protection electro-dissociator is avoided the interference that is present in the pollutant in gas to be analyzed.
However, can think to approach most known prior art solution of the present invention is disclosed ion migration frequency spectrograph in above-mentioned U.S. Patent No. 5420424.Except shortcoming described above, be that electro-dissociator is in the intrafascicular exposure of gas flow to be analyzed by the defect of the known patented technology solution of prior art.This pollution to electro-dissociator of gas because serving as reasons under analyzing, causes the unstable formation of reactive ion and also causes the electro-dissociator curent change of the time that depends on.
Summary of the invention
The object of the invention is, protection electro-dissociator is avoided by the gaseous contamination under analyzing.
Technique effect of the present invention comprises: consistency and the repeatability of improving the analysis result of gaseous medium; With the useful life that extends electro-dissociator.
Above-mentioned technique effect is because a kind of differential type ionic mobility frequency spectrograph is realized, this differential type ionic mobility frequency spectrograph comprises: cylindrical shape ionization chamber, wherein form analyte ions, ionization chamber has the import of reception gas to be analyzed and discharges the outlet of analytical gas; Ionization source; Ion eyelet; Electrode system, this electrode system comprises internal electrode and two electrodes of outer electrode of concentric locating; Analytical gap, limited by described two relative cylinder electrodes, described analytical gap has the import that receives Purge gas, and its import department by ion eyelet be used to form the regional connectivity of analyte ions, and be communicated with ion monitoring device in its exit, differential type frequency spectrograph also comprises: periodic voltage generator, and this periodic voltage generator has asymmetric polarity, and this periodic voltage generator offers outlet in the region of the nonlinear field that depends on ionic mobility; Compensating voltage source; High frequency voltage source, the increase resolution of this high frequency voltage source generator, described each parts are connected to internal electrode; Auxiliary chamber, this auxiliary chamber locates with one heart with respect to inner cylindrical electrode, described auxiliary chamber has for the import of ionized gas and outlet, and the repulsive force generator that comprises ionization source and be connected thereto, frequency spectrograph also has gas purge system, and this gas purge system is communicated in analytical gap import and auxiliary chamber's import by means of pipeline by analytical gap outlet and the outlet of ionization chamber.
Can be by radiation β source (as yttrium source) as ionization source, to form anion and cation according to frequency spectrograph of the present invention.
And, can be by electron ionization device (as corona discharge assembly) as ionization source according to frequency spectrograph of the present invention, wherein, the electrode with tip end is positioned in described auxiliary chamber, and described tip tip electrodes is connected to periodically high pressure generator.
In addition, can be by EFI day with fog as ionization source according to frequency spectrograph of the present invention, wherein, EFI day with fog capillary is positioned in described auxiliary chamber, and to carry the solution of controlled content by controlled flow, described EFI day with fog capillary is connected to DC high-voltage source.
Finally, can be by any known UV ray radiation source as ionization source according to frequency spectrograph of the present invention.
The gas purge system of frequency spectrograph of the present invention can comprise: gas flow actuator (for example, pump); Two filters, described filter is positioned in the outlet of ionization chamber and in analytical gap import; And auxiliary chamber, gas purge system also comprises three aerodynamic drag devices (pneumatic resistances), after these three aerodynamic drag devices are arranged on filter, and is positioned at the outlet for gas being discharged to atmosphere.
Brief description of the drawings
Accompanying drawing shows the schematic diagram of frequency spectrograph of the present invention.
Embodiment
According to the present invention, auxiliary Purge gas a fluid stream is flowed around electro-dissociator, this auxiliary Purge gas a fluid stream has controlled content.Then, make form reactive ion mix mutually with gas a fluid stream to be analyzed, and the ion of material to be analyzed due to heteroion recharge reaction form, these heteroions recharge react occur by reactive ion.Frequency spectrograph of the present invention comprises: ionization chamber 1; Outer cylindrical electrode 2 and inner cylindrical electrode 3, this inner cylindrical electrode 3 is located with one heart with respect to outer cylindrical electrode 2; Auxiliary chamber 4, treats a fluid stream (reacting gas) of ionized gas for receiving, this auxiliary chamber 4 locates with one heart with respect to inner cylindrical electrode 3; Ionization source 5, for example radiation β source (yttrium source), this ionization source 5 is positioned in the outlet of auxiliary chamber 4; The periodic voltage generator 6 with asymmetric polarity, this periodic voltage generator 6 provides the outlet in the region of leading to the nonlinear field that depends on ionic mobility; Compensating voltage source 7; High frequency voltage source 8, the resolution of the increase of these high frequency voltage source 8 generators, described periodic voltage generator, compensating voltage source and high frequency voltage source are connected to electrode 3; Repulsive force generator 9, this repulsive force generator is connected to chamber 4; Ion trap 10, is positioned at the end of analytical gap 11; Ion monitoring device 12 (for example galvanometer) is connected to this ion trap 10.Ionized space 13 is arranged in the outlet of chamber 4, and the region 14 that is used for forming analyte ions is arranged in chamber 1.Chamber 1 and internal electrode 3 are separated from one another, and limit ion eyelet 15, and this ion eyelet 15 makes ionic particles can move to analytical gap 11.Be provided with the import 16 that receives Purge gas, this Purge gas is led to by the wall of ionization chamber 1 and the space that electrode 2 limits.Ionization chamber 1 has the outlet 18 that receives the import 17 of gas a fluid stream to be analyzed and discharge for gas.
Frequency spectrograph is provided with gas purge system, this gas purge system by means of pipeline 19 by the outlet of the outlet of analytical gap 11 and ionization chamber 1 be communicated in the import of auxiliary chamber 4 and the import of analytical gap 11.Gas purge system comprises: gas flow actuator (for example, pump) 25; Two filters 23 and 24, are positioned at respectively in the outlet that ionizes chamber 1 and in the import of analytical gap 11; Auxiliary chamber 4; And three aerodynamic drag devices 20,21,22, after being arranged on described filter 23,24, and be positioned at for gas is discharged in the outlet of atmosphere.
Cylinder electrode and described chamber are separated from one another by supporting member 26.
Differential type frequency spectrograph is by following operation.
Under the impact of the β particle of the radiation source 5 of reactive ion in ionized space 13, be formed in ionization Purge gas a fluid stream R, this ionization Purge gas a fluid stream R comes in chamber 4.Reactive ion enters gas a fluid stream A to be analyzed, and this gas a fluid stream A comes in ionization chamber 1 through import 17.Meanwhile, a fluid stream of purification restraint gas B arrives in the space between wall and the electrode 2 of chamber 1.A part for this fluid stream arrives through ion eyelet 15 region 14 forming for analyte ions, and the other parts C of described a fluid stream goes in analytical gap 11, and this analytical gap 11 is limited by electrode 2 and 3.
The ion of analyzed material due to heteroion recharge reaction form, and by electric field from being pulled to vector gas a fluid stream C for the region forming 14 of analyte ions, this electric field is formed by the potential difference of electrode 3 and electrode 2.Ion arrives the ion trap 10 on the end in the gap 11 at different bucking voltage values place, and they are monitored by galvanometer 12, and these ions have their mobility to the different dependences of electric field strength.
Arrive cleaning system by gatherer 10 and the gas of the outlet 18 of ionization chamber 1.After purifying, an a fluid stream of Purge gas turns back to chamber 4 again, and another a fluid stream is to analytical gap 11.
Technique effect of the present invention is owing to providing pure ionized gas a fluid stream to ensure, this pure ionized gas a fluid stream prevents that analyzed " pollution " gas from contacting with ionization source.
Industrial usability
Up-to-date technique, technology and material ensure the physical possibility for the enforcement of above-mentioned differential type ionic mobility frequency spectrograph.Forming the entire infrastructure parts of frequency spectrograph can utilize current existing production facility under operation in industry and construct.There is no question about for taking technical staff in the field of environment measurement for the operability of differential type ionic mobility frequency spectrograph.
Claims (6)
1. a differential type ionic mobility frequency spectrograph, comprising: cylindrical shape ionization chamber, in described ionization chamber, form analyte ions, and ionization chamber has the import for receiving gas to be analyzed and discharges the outlet of the gas of having analyzed, ionization source, ion eyelet, electrode system, this electrode system comprises internal electrode and two electrodes of outer electrode of concentric locating, analytical gap, this analytical gap is limited by columnar contrary described two electrodes, described analytical gap has the import for receiving Purge gas, and in the import department of analytical gap by ion eyelet and the regional connectivity that is used to form analyte ions, and the exit in analytical gap is communicated with ion monitoring device, described differential type ionic mobility frequency spectrograph also comprises: have the periodic voltage generator of asymmetric polarity, this periodic voltage generator provides the outlet in the region of leading to the nonlinear field that depends on ionic mobility, compensating voltage source, high frequency voltage source, the resolution of the increase of this high frequency voltage source generator, described each parts are connected to internal electrode, it is characterized in that, described frequency spectrograph has auxiliary chamber, this auxiliary chamber locates with one heart with respect to columnar internal electrode, described auxiliary chamber has for the import of ionized gas and outlet, described auxiliary chamber holds ionization source and is connected to the repulsive force generator of described auxiliary chamber, described frequency spectrograph also has gas purge system, this gas purge system is communicated in the import of analytical gap and the import of auxiliary chamber by means of pipeline by the outlet of the outlet of analytical gap and ionization chamber.
2. frequency spectrograph according to claim 1, is characterized in that, by radiation β source, as ionization source, described radiation β source is for example yttrium source.
3. frequency spectrograph according to claim 1, it is characterized in that, electron ionization device is used as to described ionization source, wherein, the electrode with tip end is positioned in described auxiliary chamber, the described electrode with tip end is connected to cycle high pressure generator, and described electron ionization device is for example corona discharge assembly.
4. frequency spectrograph according to claim 1, is characterized in that, EFI day with fog is used as to ionization source, wherein, EFI day with fog capillary is positioned in described auxiliary chamber, to carry the solution of controlled content with controlled flow, described EFI day with fog capillary is connected to DC high-voltage source.
5. frequency spectrograph according to claim 1, is characterized in that, any known UV ray radiation source is used as to ionization source.
6. frequency spectrograph according to claim 1, is characterized in that, gas purge system comprises: gas flow actuator (for example, pump); Two filters, described two filters are positioned in the outlet that ionizes chamber and in the import of analytical gap; And auxiliary chamber, gas purge system also comprises three aerodynamic drag devices, these three aerodynamic drag devices are arranged on filter afterwards and are positioned at for the outlet to atmosphere by gas discharging.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2012121133/07A RU2503083C1 (en) | 2012-05-22 | 2012-05-22 | Differential ion mobility spectrometer |
| RU2012121133 | 2012-05-22 | ||
| PCT/RU2013/000359 WO2013176580A1 (en) | 2012-05-22 | 2013-04-25 | Differential ion mobility spectrometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104054156A true CN104054156A (en) | 2014-09-17 |
| CN104054156B CN104054156B (en) | 2016-06-15 |
Family
ID=49624156
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201380004790.4A Expired - Fee Related CN104054156B (en) | 2012-05-22 | 2013-04-25 | Differential type mobility of ions spectrometer |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN104054156B (en) |
| DE (1) | DE112013000365B4 (en) |
| RU (1) | RU2503083C1 (en) |
| WO (1) | WO2013176580A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017101285A1 (en) * | 2015-12-15 | 2017-06-22 | 清华大学深圳研究生院 | Tracing method for distribution of mobile ions in ionic migration spectrometer |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2577781C1 (en) * | 2014-09-09 | 2016-03-20 | Закрытое акционерное общество "Инновационный центр "Бирюч" (ЗАО "ИЦ "Бирюч") | Ion mobility differential spectrometer of ion trap |
| RU2620251C2 (en) * | 2015-08-21 | 2017-05-24 | Закрытое акционерное общество "Инновационный центр "Бирюч" (ЗАО "ИЦ "Бирюч") | Differential ion mobility spectrometer with a laminar flow |
| CN108091541B (en) * | 2016-11-21 | 2019-09-06 | 中国科学院大连化学物理研究所 | A kind of array High-Field asymmetric waveform transference tube |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5420424A (en) * | 1994-04-29 | 1995-05-30 | Mine Safety Appliances Company | Ion mobility spectrometer |
| RU2150157C1 (en) * | 1998-06-09 | 2000-05-27 | Конструкторско-технологический институт геофизического и экологического приборостроения СО РАН | Spectrometer of nonlinearity of drift of ions |
| JP2000509487A (en) * | 1996-04-04 | 2000-07-25 | マイン・セイフティ・アプライアンセス・カンパニー | Recirculating filtration device for use with a portable ion mobility analyzer |
| RU2178929C2 (en) * | 2000-01-25 | 2002-01-27 | Конструкторско-технологический институт геофизического и экологического приборостроения СО РАН | Spectrometer of non-linearity of drift of ions |
| US20090114811A1 (en) * | 2007-11-06 | 2009-05-07 | Jurgen Landgraf | Ion mobility spectrometer and method for operation |
| US20100282961A1 (en) * | 2007-02-01 | 2010-11-11 | Sionex Corporation | Differential mobility spectrometer pre-filter assembly for a mass spectrometer |
| CN102046833A (en) * | 2008-05-30 | 2011-05-04 | 应用材料股份有限公司 | Arrangement and method for removing alkali- or alkaline earth-metals from a vacuum coating chamber |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5801379A (en) * | 1996-03-01 | 1998-09-01 | Mine Safety Appliances Company | High voltage waveform generator |
| US5736739A (en) * | 1996-04-04 | 1998-04-07 | Mine Safety Appliances Company | Recirculating filtration system for use with a transportable ion mobility spectrometer in gas chromatography applications |
| DE102005004325A1 (en) * | 2005-01-31 | 2006-08-10 | Bruker Daltonik Gmbh | Ion mobility spectrometer and method of its operation |
-
2012
- 2012-05-22 RU RU2012121133/07A patent/RU2503083C1/en active
-
2013
- 2013-04-25 CN CN201380004790.4A patent/CN104054156B/en not_active Expired - Fee Related
- 2013-04-25 DE DE112013000365.1T patent/DE112013000365B4/en not_active Expired - Fee Related
- 2013-04-25 WO PCT/RU2013/000359 patent/WO2013176580A1/en active Application Filing
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5420424A (en) * | 1994-04-29 | 1995-05-30 | Mine Safety Appliances Company | Ion mobility spectrometer |
| JP2000509487A (en) * | 1996-04-04 | 2000-07-25 | マイン・セイフティ・アプライアンセス・カンパニー | Recirculating filtration device for use with a portable ion mobility analyzer |
| RU2150157C1 (en) * | 1998-06-09 | 2000-05-27 | Конструкторско-технологический институт геофизического и экологического приборостроения СО РАН | Spectrometer of nonlinearity of drift of ions |
| RU2178929C2 (en) * | 2000-01-25 | 2002-01-27 | Конструкторско-технологический институт геофизического и экологического приборостроения СО РАН | Spectrometer of non-linearity of drift of ions |
| US20100282961A1 (en) * | 2007-02-01 | 2010-11-11 | Sionex Corporation | Differential mobility spectrometer pre-filter assembly for a mass spectrometer |
| US20090114811A1 (en) * | 2007-11-06 | 2009-05-07 | Jurgen Landgraf | Ion mobility spectrometer and method for operation |
| CN102046833A (en) * | 2008-05-30 | 2011-05-04 | 应用材料股份有限公司 | Arrangement and method for removing alkali- or alkaline earth-metals from a vacuum coating chamber |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017101285A1 (en) * | 2015-12-15 | 2017-06-22 | 清华大学深圳研究生院 | Tracing method for distribution of mobile ions in ionic migration spectrometer |
| US10161904B2 (en) | 2015-12-15 | 2018-12-25 | Graduate School At Shenzhen, Tsinghua University | Method for tracing distribution of moving ions in ion mobility spectrometer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104054156B (en) | 2016-06-15 |
| WO2013176580A1 (en) | 2013-11-28 |
| RU2012121133A (en) | 2013-12-10 |
| DE112013000365B4 (en) | 2016-07-14 |
| RU2503083C1 (en) | 2013-12-27 |
| DE112013000365T5 (en) | 2014-10-02 |
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